Thiol ester acid and preparation method and application thereof

A mercapto acid and esterification technology, which is applied in the field of preparing thermoreversible ion-crosslinked polyvinyl chloride, can solve problems such as difficult industrialization, and achieve the effects of avoiding the precipitation of additives, inhibiting coloring and degradation, and achieving good compatibility.

Active Publication Date: 2015-01-14
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Although it is a feasible way to prepare thermally reversible ion-c

Method used

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  • Thiol ester acid and preparation method and application thereof
  • Thiol ester acid and preparation method and application thereof
  • Thiol ester acid and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Under the protection of oxygen-free and high-purity nitrogen (purity ≥ 99.999%), mix 117 grams of adipic acid (analytical grade), 70 grams of mercaptoethanol (analytic grade) and 200 grams of xylene (analytic grade) and stir , and then gradually heated the temperature from room temperature to 130°C; after the adipic acid was melted and dissolved, a solution prepared by 1 gram of p-toluenesulfonic acid (analytical pure) and 50 grams of toluene was added dropwise, under oxygen-free and high-purity nitrogen atmosphere Under protection, the esterification reaction was carried out at a temperature of 130° C. for 6 hours, and at the same time, the water generated by the reaction was received in the water separator. After the product is cooled for several hours, remove the sediment, take the upper layer solution and evaporate toluene and xylene under reduced pressure to obtain 148 grams of colorless, transparent and viscous mercaptoesteric acid; add 10 grams of anhydrous Magne...

Embodiment 2

[0067] 100 grams of DOP and 50 grams of light magnesium oxide are added to an emulsifier, and ground into a slurry at room temperature; two parts of each 13.5 grams of the above-mentioned grinding slurry are respectively added at room temperature. 1 prepare the mercaptoesteric acid, then add 1 gram and 21 grams of DOP and mix respectively to obtain composite slurry (the total content of DOP in the two kinds of composite slurry is respectively 10 grams and 30 grams); then to the composite slurry Add 100 grams of polyvinyl chloride resin with a degree of polymerization of 1000 in each material, knead with a high-speed mixer at 25 ° C, and obtain a polyvinyl chloride dry mixture after cooling; the obtained polyvinyl chloride dry mixture is passed through a double-roller open mill Molded for 5 minutes, the temperature during mastication was 150°C, and two 0.8mm-thick samples with different DOP amounts were obtained, and then the three-layer samples were stacked under a single-layer...

Embodiment 3

[0072] Get 13.5 grams of grinding slurry in Example 2, add 4.5 grams of mercaptoesteric acid prepared in Example 1 and 1 gram of DOP at room temperature and stir and mix, then add 100 grams of polyvinyl chloride resin with a degree of polymerization of 1000, at 25 ° C Knead with a high-speed mixer and cool to obtain a polyvinyl chloride dry mix; the obtained polyvinyl chloride dry mix is ​​masticated by a double-roller mill for 5 minutes to obtain a sample. The temperature during mastication is 170 ° C, and then three layers The samples were stacked under a single-layer electric tablet press at 180°C, and hot-pressed at a temperature of 180°C for 10 minutes to make a 2mm thick thermoreversible ion-crosslinked polyvinyl chloride sample. The appearance of the sample can be seen Figure 4 C in

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Abstract

The invention relates to a thiol ester acid and a preparation method and application thereof. The thiol ester acid with the molecular formula of HOOC-R1-COO-R2-SH is prepared by full esterification reaction of a dicarboxylic acid and thiol in the presence of a catalyst under oxygen-free environment, the thiol ester acid and light magnesium oxide as synergic crosslinking agents and a plasticizer and a lead-free stabilizer are together used for the preparation of composite slurry, and the composite slurry is used for the preparation of thermally reversible ionic crosslinking polyvinyl chloride. In the use of the composite slurry prepared by the preparation method, the synergic crosslinking agents formed by the thiol ester acid and the light magnesium oxide bonds thiol group onto the side group of a PVC (polyvinyl chloride) molecular chain by chlorine atom replacement, and a carboxylic acid and alkaline earth metal ion cluster is formed, the mechanical properties of PVC can be improved, the thermoplasticity can be maintained, coloring and degradation in the PVC plasticization process can be inhibited, and preparation of thermally reversible ionic crosslinking PVC in the plasticization and processing molding and cooling shaping process can be realized.

Description

technical field [0001] The invention relates to a mercaptoester acid and a preparation method thereof, and the composite of the mercaptoester acid and light magnesium oxide is used as a crosslinking agent for preparing thermally reversible ion-crosslinked polyvinyl chloride. Background technique [0002] The mechanical properties and heat distortion temperature of thermoplastic polyvinyl chloride (PVC) will be significantly improved after cross-linking. Many cross-linking technologies have been reported in the existing literature, such as the literature ("Research Progress in PVC Cross-linking Technology", PVC Ethylene, 2005, 3:7). The traditional cross-linking technology mostly connects linear polymer molecules into a stable three-dimensional network, resulting in the loss of the original thermoplasticity. In recent years, a new technology called thermoreversible crosslinking has been paid more and more attention. The thermally reversible cross-linked polymer obtained by ...

Claims

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Application Information

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IPC IPC(8): C07C323/12C07C319/12C08L27/06C08K13/02C08K5/37C08K3/22C08J3/24
Inventor 刘晓明马永梅
Owner INST OF CHEM CHINESE ACAD OF SCI
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